CN111620345A - Superfine hydrophobic silicon dioxide and preparation method thereof - Google Patents
Superfine hydrophobic silicon dioxide and preparation method thereof Download PDFInfo
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- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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Abstract
The invention belongs to the technical field of silicon dioxide, and particularly relates to superfine hydrophobic silicon dioxide and a preparation method thereof. The invention adopts sodium silicate solution and sulfuric acid solution to react at 70-80 ℃ to prepare silicon dioxide material, and after washing and drying, the silicon dioxide is synchronously subjected to superfine grinding and modification in an airflow mill to prepare the superfine hydrophobic silicon dioxide. The superfine hydrophobic silicon dioxide provided by the invention has the advantages of uniform appearance and particle size, good hydrophobic effect and high transparency. The preparation method of the superfine hydrophobic silica provided by the invention is simple and easy to operate, is safe and environment-friendly, can realize continuous production, and is low in production cost.
Description
Technical Field
The invention belongs to the technical field of silicon dioxide, and particularly relates to superfine hydrophobic silicon dioxide and a preparation method thereof.
Background
Hydrophobic materials generally refer to materials having a contact angle of water at a static surface of greater than 90 °. Due to good non-wettability to water, the hydrophobic material generally has excellent self-cleaning, pollution resistance, corrosion resistance and other properties, and has wide application prospects in daily life and many industrial fields.
China is a large country for paint production and consumption, but the current domestic paint generally has the defects in performance, such as poor suspension stability, poor thixotropy, poor weather resistance, poor scrub resistance and the like, so that a large amount of high-quality paint needs to be imported every year, and the paint cost is high. After the super-hydrophobic silicon dioxide is applied to the coating, the defects of the conventional product can be overcome, the performance indexes of the coating are greatly improved except that the contrast ratio is unchanged, for example, the washing resistance of the exterior wall coating is improved from thousands of times to ten thousands of times, the time for artificially accelerating weather aging and artificial radiation exposure aging is improved from 250 hours to 600 hours, in addition, the bonding strength of a coating and a wall body is greatly improved, the hardness of the coating is obviously improved, and the surface self-cleaning capability is also improved.
Application publication No. CN104876230A discloses a method for preparing monodisperse ordered hydrophobic silica nanoparticles, which comprises the following steps: firstly, a mixed solution prepared from a surfactant, a prepolymer, water and ethanol is placed in a beaker and stirred for 6 hours below 30 ℃. The mixed solution was poured into a flask, and a certain amount of benzene was added to form a microemulsion, which was stirred at 69 ℃ for 1 hour. The temperature was then adjusted to 105 ℃ until water and ethanol were completely distilled off. And drying the residual solution to obtain a powder sample, adding the mixed washing solution, carrying out high-speed centrifugation, and drying the precipitate below the centrifugal tube at 60 ℃. And collecting the dried product to obtain the monodisperse nano-pore hydrophobic silicon dioxide with uniform size. The hydrophobic silicon dioxide prepared by the preparation method has the advantages of complex preparation method, more reagent types and higher production cost.
In conclusion, the prior art has various technical problems of complex preparation method, various reagent types, high production cost, poor safety and environmental protection performance and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the ultrafine hydrophobic silica and the preparation method thereof. The preparation method of the superfine hydrophobic silicon dioxide simplifies the preparation process of the hydrophobic silicon dioxide, reduces the production cost, improves the production yield, and is safe and environment-friendly.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of ultrafine hydrophobic silica specifically comprises the following steps:
s1, adding a sodium silicate solution with the molar concentration of 0.45-0.65mol/L into a reaction tank, heating to 70-80 ℃ by using steam, starting a stirring device, dripping a dilute sulfuric acid solution with the molar concentration of 1.0-1.5mol/L under the condition of stirring frequency of 30-40Hz, and controlling the pH value of a reaction end point to be 3.5-6.0 to prepare a mixed solution A;
s2, performing filter pressing washing and flash evaporation drying on the mixed liquid A prepared in the step S1, and pumping the mixed liquid A into a buffer tank to prepare a dry material;
s3, opening the airflow flour mill, controlling the speed of the grading wheel to 1400-1600rpm, opening the high-temperature air compressor, and pumping high-temperature air;
and S4, spraying the dry material prepared in the step S2 and the silane coupling agent into an airflow mill, and carrying out physical crushing through high-temperature high-pressure gas for 30min to obtain the silane coupling agent.
Further, the adding amount of the sodium silicate solution in the step S1 is 10-15m3The dropping speed of the dilute sulfuric acid solution is 2-4m3/h。
Further, in the step S2, feeding for 12-16min under the condition that the pressure in the pressure filtration process is kept at 1.6-2.0Mpa, the washing time is 80-160min, and the washing conductivity is 2000-; the inlet temperature of the flash drying is 350-550 ℃, and the outlet temperature is 100-130 ℃.
Further, the temperature of the high temperature air in the step S3 is 200-250 ℃.
Further, the feeding speed of the dry material in the step S4 is 2-3 t/h.
Further, the percentage concentration of the silane coupling agent solution in the step S4 is 0.5-10%; the feeding speed of the silane coupling agent is 0.2-0.3 t/h.
Further, the airflow mill in the step S3 is connected to a high-temperature air compressor, and the liquid pipe of the ejector is connected to a silane coupling agent.
The invention also provides the superfine hydrophobic silicon dioxide prepared by the preparation method.
The invention adopts sodium silicate solution and sulfuric acid solution to react at 70-80 ℃ to prepare silicon dioxide material, and after washing and drying, the silicon dioxide is synchronously subjected to superfine grinding and modification in an airflow mill to prepare the superfine hydrophobic silicon dioxide. The invention controls the reaction end point of the sodium silicate solution and the sulfuric acid solution, so that the generated silicon dioxide particles are loose and porous and have higher transparency.
After the silicon dioxide particles are fully contacted with the silane coupling agent in the airflow mill, the silane coupling agent can be adsorbed on the surface of the silicon dioxide particles, so that a plurality of small bulges are formed on the surface of the silicon dioxide particles, a small air chamber with one is formed in the middle of each bulge, a special micro-nano structure is formed, after the superfine hydrophobic silicon dioxide is added into the coating, water drops are large in size and cannot enter the small air chambers, and the hydrophobic property of the superfine hydrophobic silicon dioxide is improved.
In addition, the superfine hydrophobic silica with uniform appearance, particle size and weight can be separated by a higher classifying wheel speed in the airflow mill, so that the worthy superfine hydrophobic silica has uniform particle size and better performance. The raw materials in the preparation process of the superfine hydrophobic silica only comprise a sodium silicate solution, a sulfuric acid solution and a silane coupling agent, so that the types of the hydrophobic silica reaction raw materials in the prior art are greatly reduced, the production cost is greatly reduced, and the sodium silicate solution, the dilute sulfuric acid solution and the silane coupling agent are harmless to human bodies and environment-friendly, so that the safety and environmental friendliness are greatly improved.
Compared with the prior art, the superfine hydrophobic silicon dioxide and the preparation method thereof provided by the invention have the following advantages:
(1) the hydrophobic silicon dioxide prepared by the invention has uniform particle size, good hydrophobic effect and high transparency;
(2) the preparation method of the hydrophobic silicon dioxide provided by the invention is simple, the conditions are controllable, and the industrial production is easy to realize;
(3) the preparation method of the hydrophobic silicon dioxide provided by the invention has the advantages of less reaction raw materials and good environmental protection performance, reduces the production cost of the hydrophobic silicon dioxide, and improves the technical problem of poor safety and environmental protection.
Detailed Description
The present invention will be further described below by way of specific embodiments, but the present invention is not limited to only the following examples. Various modifications can be made by those skilled in the art based on the basic idea of the invention, but it is within the scope of the invention as long as it does not depart from the basic idea of the invention.
The air current milling machine in this embodiment is connected with the high-temperature air compressor, and the liquid pipe of the ejector is connected with the silane coupling agent.
Example 1 preparation of ultra-fine hydrophobic silica
A preparation method of ultrafine hydrophobic silica specifically comprises the following steps:
s1, adding 10m into the reaction tank3Heating sodium silicate solution with molar concentration of 0.45mol/L to 77 deg.C with steam, starting stirring device, and stirring at stirring frequency of 30Hz by 2m3Dripping dilute sulfuric acid solution with the molar concentration of 1.0mol/L at the speed of/h, and controlling the pH value of the reaction end point to be 3.5 to prepare mixed liquid A;
s2, performing filter pressing washing and flash evaporation drying on the mixed liquid A prepared in the step S1, pumping the mixed liquid A into a buffer tank, feeding for 12min under the condition that the pressure is kept at 2.0Mpa in the filter pressing process, wherein the washing time is 160min, and the washing conductivity is 2000 mu S/cm; the inlet temperature of flash drying is 350 ℃, the outlet temperature is 100 ℃ to prepare a dry material;
s3, opening the airflow flour mill, controlling the speed of the grading wheel to 1450rpm, opening the high-temperature air compressor, and pumping high-temperature air with the temperature of 200 ℃;
and S4, spraying the dry material prepared in the step S2 and a silane coupling agent solution with the percentage concentration of 8% into an airflow grinding mill, wherein the spraying speed of the dry material is 2.2t/h, the spraying speed of the silane coupling agent is 0.28t/h, and performing physical crushing through high-temperature high-pressure gas and keeping for 30min to obtain the silane coupling agent.
Example 2 preparation method of ultra-fine hydrophobic silica
A preparation method of ultrafine hydrophobic silica specifically comprises the following steps:
s1, adding 11m into the reaction tank3Heating sodium silicate solution with molar concentration of 0.5mol/L to 73 deg.C with steam, starting stirring device, and stirring at stirring frequency of 32Hz by 2.5m3Dripping dilute sulfuric acid solution with the molar concentration of 1.2mol/L at the speed of/h, and controlling the pH value of the reaction end point to be 4.0 to prepare mixed liquid A;
s2, performing filter pressing washing and flash evaporation drying on the mixed liquid A prepared in the step S1, pumping the mixed liquid A into a buffer tank, feeding for 13min under the condition that the pressure is kept at 1.9Mpa in the filter pressing process, wherein the washing time is 140min, and the washing conductivity is 3000 mu S/cm; the inlet temperature of flash drying is 400 ℃, the outlet temperature is 105 ℃, and a dry material is prepared;
s3, opening the airflow flour mill, controlling the speed of a grading wheel to be 1600rpm, opening a high-temperature air compressor, and pumping high-temperature air with the temperature of 220 ℃;
and S4, spraying the dry material prepared in the step S2 and a silane coupling agent solution with the percentage concentration of 6% into an airflow grinding mill, wherein the spraying speed of the dry material is 2.8t/h, the spraying speed of the silane coupling agent is 0.24t/h, and performing physical crushing through high-temperature high-pressure gas and keeping for 30min to obtain the silane coupling agent.
Example 3 preparation of ultra-fine hydrophobic silica
A preparation method of ultrafine hydrophobic silica specifically comprises the following steps:
s1, adding 12.5m into the reaction tank3Heating sodium silicate solution with molar concentration of 0.55mol/L to 80 deg.C with steam, starting stirring device, and stirring at stirring frequency of 35Hz by 3m3Dripping dilute sulfuric acid solution with the molar concentration of 1.3mol/L at the speed of/h, and controlling the pH value of the reaction end point to be 4.5 to prepare mixed liquid A;
s2, performing filter pressing washing and flash evaporation drying on the mixed liquid A prepared in the step S1, pumping the mixed liquid A into a buffer tank, feeding for 14min under the condition that the pressure is kept at 1.8Mpa in the filter pressing process, wherein the washing time is 110min, and the washing conductivity is 4000 mu S/cm; the inlet temperature of flash drying is 450 ℃, and the outlet temperature is 115 ℃ to prepare a dry material;
s3, opening the airflow flour mill, controlling the speed of the classification wheel to be 1500rpm, opening the high-temperature air compressor, and pumping high-temperature air with the temperature of 230 ℃;
and S4, spraying the dry material prepared in the step S2 and the silane coupling agent solution with the percentage concentration of 10% into an airflow grinding mill, wherein the spraying speed of the dry material is 2.0t/h, the spraying speed of the silane coupling agent is 0.30t/h, and performing physical crushing through high-temperature high-pressure gas and keeping for 30min to obtain the silane coupling agent.
Example 4 preparation of ultra-fine hydrophobic silica
A preparation method of ultrafine hydrophobic silica specifically comprises the following steps:
s1, adding 14m into the reaction tank3Heating sodium silicate solution with molar concentration of 0.6mol/L to 78 deg.C with steam, starting stirring device, and stirring at stirring frequency of 37Hz by 3.5m3Dripping dilute sulfuric acid solution with the molar concentration of 1.4mol/L at the speed of/h, and controlling the pH value of the reaction end point to be 5.0 to prepare mixed liquid A;
s2, performing filter pressing washing and flash evaporation drying on the mixed liquid A prepared in the step S1, pumping the mixed liquid A into a buffer tank, feeding for 15min under the condition that the pressure is kept at 1.7Mpa in the filter pressing process, wherein the washing time is 90min, and the washing conductivity is 5000 mus/cm; the inlet temperature of flash evaporation drying is 500 ℃, and the outlet temperature is 120 ℃, so as to prepare a dry material;
s3, opening the airflow flour mill, controlling the speed of the classification wheel to 1400rpm, opening the high-temperature air compressor, and pumping high-temperature air with the temperature of 240 ℃;
and S4, spraying the dry material prepared in the step S2 and a silane coupling agent solution with the percentage concentration of 0.5% into an airflow pulverizer, wherein the spraying speed of the dry material is 3.0t/h, the spraying speed of the silane coupling agent is 0.20t/h, and physically crushing the dry material and the silane coupling agent solution through high-temperature high-pressure gas and keeping the crushed dry material and the silane coupling agent solution for 30min to obtain the silane coupling agent.
Example 5 preparation of ultra-fine hydrophobic silica
A preparation method of ultrafine hydrophobic silica specifically comprises the following steps:
s1, adding 15m into the reaction tank3Heating sodium silicate solution with molar concentration of 0.65mol/L to 70 deg.C with steam, starting stirring device, and stirring at stirring frequency of 40Hz by 4m3Dripping dilute sulfuric acid solution with the molar concentration of 1.5mol/L at the speed of/h, and controlling the pH value of the reaction end point to be 6 to prepare mixed solution A;
s2, performing filter pressing washing and flash evaporation drying on the mixed liquid A prepared in the step S1, pumping the mixed liquid A into a buffer tank, feeding for 16min under the condition that the pressure is kept at 1.6Mpa in the filter pressing process, wherein the washing time is 80min, and the washing conductivity is 6000 mus/cm; the inlet temperature of flash drying is 550 ℃, and the outlet temperature is 130 ℃ to prepare a dry material;
s3, opening the airflow flour mill, controlling the speed of a grading wheel to be 1550rpm, opening a high-temperature air compressor, and pumping high-temperature air with the temperature of 250 ℃;
and S4, spraying the dry material prepared in the step S2 and a silane coupling agent solution with the percentage concentration of 6% into an airflow grinding mill, wherein the spraying speed of the dry material is 2.4t/h, the spraying speed of the silane coupling agent is 0.22t/h, and performing physical crushing through high-temperature high-pressure gas and keeping for 30min to obtain the silane coupling agent.
Comparative example 1 preparation method of ultrafine hydrophobic silica
The preparation of the ultra-fine hydrophobic silica in this comparative example was similar to that of example 3.
The difference between this comparative example and example 3 is: the reaction end point of the sodium silicate solution and the sulfuric acid solution was controlled to 6.5 in step S1 of this comparative example.
Comparative example 2 preparation method of ultrafine hydrophobic silica
The preparation of the ultra-fine hydrophobic silica in this comparative example was similar to that of example 3.
The difference between this comparative example and example 3 is: in step S4 of this comparative example, the silane coupling agent was replaced with a phthalate coupling agent.
Comparative example 3 preparation method of ultrafine hydrophobic silica
The preparation of the ultra-fine hydrophobic silica in this comparative example was similar to that of example 3.
The difference between this comparative example and example 3 is: the classification wheel speed in step S3 of this comparative example was 600 rpm.
Test example, ultra-fine hydrophobic silica Performance test
Test samples: ultrafine hydrophobic silica and ordinary silica prepared in examples 1 to 5 and comparative examples 1 to 3;
the test method comprises the following steps: detecting the particle size of the superfine hydrophobic silica: detecting the average particle size of a test sample by using a high-performance specific surface area analyzer (the brand is Jing-Gaobao, and the model is JW-BK 200);
and (3) detecting the transparency of the superfine hydrophobic silica: respectively weighing 0.5 +/-0.01 g of superfine hydrophobic silica in a glass bottle, taking 12.0 +/-0.01 g of sorbitol/water mixed solution in a sterile glass bottle, and fully stirring to uniformly disperse the silica in the sorbitol/water mixed solution; placing the glass bottle in a vacuum drier, vacuumizing by using a vacuum pump, and keeping the vacuum for 0.5 h; the vacuum was released and the sample was taken out of the desiccator, visual inspection was carried out to ensure that the air in the sample had been completely removed, and the dispersion was immediately tested for transparency at a wavelength of 589 nm;
and (3) detecting the hydrophobic property of the superfine hydrophobic silica: the test samples were coated on a glass slide at 25 deg.C, 5. mu.L of water droplets were dropped on the slide, the contact angle of the ultra-fine hydrophobic silica was measured by a contact angle measuring instrument (DSA100, KRUSS, Germany), 10 test points were taken for each sample, the maximum angle and the minimum angle were removed, and the average value was taken as the measured value of the sample.
And (3) test results: the test results are shown in Table 1.
TABLE 1 Performance testing of ultra-fine hydrophobic silicas
As can be seen from Table 1, the average particle size of the ultrafine hydrophobic silica provided by the invention is 3-8 μm, the transparency is 95-99%, and the contact angle is 141-159 degrees. Among them, the ultra-fine hydrophobic silica prepared in example 3 has the greatest transparency and contact angle and the best transparency and hydrophobicity, and is the best example of the present invention.
The ultra-fine hydrophobic silicas prepared in comparative examples 1-3 had reduced transparency and varied contact angles compared to example 3, indicating that the process for preparing the ultra-fine hydrophobic silica provided by the present invention has been flow-optimized.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art will recognize that changes may be made to the embodiments described above without departing from the spirit and scope of the invention. Therefore, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the technical spirit of the present invention are covered by the claims of the present invention.
Claims (8)
1. The preparation method of the superfine hydrophobic silica is characterized by comprising the following steps:
s1, adding a sodium silicate solution with the molar concentration of 0.45-0.65mol/L into a reaction tank, heating to 70-80 ℃ by using steam, starting a stirring device, dripping a dilute sulfuric acid solution with the molar concentration of 1.0-1.5mol/L under the condition of stirring frequency of 30-40Hz, and controlling the pH value of a reaction end point to be 3.5-6.0 to prepare a mixed solution A;
s2, performing filter pressing washing and flash evaporation drying on the mixed liquid A prepared in the step S1, and pumping the mixed liquid A into a buffer tank to prepare a dry material;
s3, opening the airflow flour mill, controlling the speed of the grading wheel to 1400-1600rpm, opening the high-temperature air compressor, and pumping high-temperature air;
and S4, spraying the dry material prepared in the step S2 and the silane coupling agent into an airflow mill, and carrying out physical crushing through high-temperature high-pressure gas for 30min to obtain the silane coupling agent.
2. The method for preparing ultra-fine hydrophobic silica according to claim 1, wherein the sodium silicate solution is added in an amount of 10-15m in the step S13The dropping speed of the dilute sulfuric acid solution is 2-4m3/h。
3. The method as claimed in claim 1, wherein the pressure filtration process in step S2 is performed under a pressure of 1.6-2.0Mpa for 12-16min, the washing time is 80-160min, and the washing conductivity is 2000-; the inlet temperature of the flash drying is 350-550 ℃, and the outlet temperature is 100-130 ℃.
4. The method as claimed in claim 1, wherein the temperature of the high temperature air in the step S3 is 200-250 ℃.
5. The method for preparing ultra-fine hydrophobic silica according to claim 1, wherein the feeding speed of the dry material in the step S4 is 2-3 t/h.
6. The method for preparing ultra-fine hydrophobic silica as claimed in claim 1, wherein the percentage concentration of the silane coupling agent solution in the step S4 is 0.5-10%; the feeding speed of the silane coupling agent is 0.2-0.3 t/h.
7. The method of claim 1, wherein the jet mill of step S3 is connected to a high temperature air compressor, and the silane coupling agent is connected to the injector liquid pipe.
8. An ultra-fine hydrophobic silica prepared by the method for preparing an ultra-fine hydrophobic silica according to any one of claims 1 to 7.
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| CN112226221A (en) * | 2020-10-19 | 2021-01-15 | 河南大学 | Nano silicon dioxide oil displacement agent and preparation method and application thereof |
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Application publication date: 20200904 |